Synthesis and crystal structure analysis of trichloro(dimethylformamide)bis(dimethylsulfoxide)rhodium(III)

1983 ◽  
Vol 61 (8) ◽  
pp. 1823-1826 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
R. Melanson
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Dmso Molecule ◽  
Crystal Structure Analysis ◽  
Trans Position ◽  
Synthesis And Crystal Structure ◽  
Full Matrix ◽  
R Factor ◽  
In Trans

mer-[Rh(DMSO)2(DMF)Cl3] was prepared by dissolving [Rh(DMSO)3Cl3] in dimethylformamide (DMF). It forms monoclinic crystals, a = 11.530(3), b = 8.971(2), c = 15.912(3) Å, β = 107.88(2)°, Z = 4, and space group P21/c. The structure was refined by full-matrix least-squares analysis to a conventional R factor of 0.038 (3495 observed reflections).The coordination around the Rh atom is octahedral. The compound is the peripheral or the 1,2,6-isomer. The DMF molecule is in trans position to a DMSO ligand and bonded to rhodium through the oxygen atom. The two molecules of DMSO are bonded to rhodium through sulfur. The Rh—Cl(1) bond (2.366(1) Å) trans to a DMSO molecule seems slightly longer than the two Rh—Cl bonds trans to each other (2.329(1) and 2.343(1) Å).

The molecular and crystal structure of trans-dichloro(dimethylformamide) (2,6-lutidine)platinum(II)

1980 ◽  
Vol 58 (2) ◽  
pp. 97-101 ◽  
Author(s):  
F. D. Rochon ◽  
P. C. Kong ◽  
R. Melanson
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Pyridine Derivative ◽  
X Ray Diffraction ◽  
Orthorhombic Space Group ◽  
Full Matrix ◽  
X Ray ◽  
R Factor ◽  
Square Planar

The crystal structure of trans-[Pt(DMF)(2,6-lutidine)Cl2] has been determined by X-ray diffraction. The crystals are orthorhombic, space group Pbca, with a = 11.612(13), b = 26.504(33), c = 9.271(9) Å, and Z = 8. The structure was refined by full matrix least-squares analysis to a conventional R factor of 0.051 and a weighted Rw = 0.044. The coordination around the platinum atom is square planar. The 2,6-lutidine ring is perpendicular to the platinum plane. DMF is bonded to platinum through the oxygen atom. It is planar and makes an angle of 71 ° with the platinum plane. The cis–trans configuration of the [Pt(DMF)(L)Cl2] (L = pyridine derivative) complexes in DMF solution is discussed.

Refinement of the structure of Mg2As2O7

1970 ◽  
Vol 48 (6) ◽  
pp. 890-894 ◽  
Author(s):  
C. Calvo ◽  
K. Neelakantan
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Unit Cell ◽  
Full Matrix ◽  
Space Group ◽  
Cell Dimensions ◽  
Central Oxygen ◽  
R Value ◽  
Unit Cell Dimensions

The crystal structure of Mg2As2O7 has been refined by full matrix least squares procedures using 587 observed reflections. The structure of Mg2As2O7 is of the thortveitite type, as reported by Łukaszewicz, with space group C2/m and unit cell dimensions a = 6.567(2) Å, b = 8.524(4) Å, c = 4.739(1) Å, β = 103.8(1)°, and Z = 2. The As—O—As group in the anion appears to be linear but the central oxygen atom undergoes considerable disorder in the plane perpendicular to this group. The AsO bond distances uncorrected for thermal motion are 1.67 Å for the As—O(—As) bond and 1.66 and 1.65 Å for the terminal As—O bonds. The final R value obtained is 0.088.

Crystal Structure of α-VPO5

1973 ◽  
Vol 51 (16) ◽  
pp. 2621-2625 ◽  
Author(s):  
Byron Jordan ◽  
Crispin Calvo
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Least Squares Method ◽  
Fold Axis ◽  
Full Matrix ◽  
Bond Lengths ◽  
R Value ◽  
A Site ◽  
Vanadium Ion

α-VPO5 crystallizes in the tetragonal space group P4/n with a = 6.014(7) and c = 4.434(2) Å. The structure, isotypic with that of α-VSO5, was refined by full-matrix least-squares method to an R value of 0.089 using 239 independent reflections. The vanadium ion lies on a crystallographic four-fold axis, as does one of the oxygen atoms, and the P on a site of [Formula: see text] symmetry. A second oxygen atom, as a result of disorder, occurs in two positions which are mirror reflected with respect to the ac plane. The structure consists of highly distorted VO6 groups with bond lengths along the c axis of 1.580(11) and 2.853(11) Å while the remaining four V—O bond lengths are all 1.858(8) Å. The P—O bond lengths in the PO4. tetrahedron are 1.541(8) Å with the PO4 groups bridging across four chains of VO6 groups.

The Crystal Structure of cis-Dichloro(2,2′-oxydi-3-butene)platinum(II), PtCl2((CH2=CH—CH(CH3))2O)

1973 ◽  
Vol 51 (4) ◽  
pp. 604-608 ◽  
Author(s):  
J. Hubert ◽  
A. L. Beauchamp ◽  
T. Theophanides
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Platinum Atom ◽  
Double Bonds ◽  
Triclinic Space Group ◽  
Standard Methods ◽  
Full Matrix ◽  
R Factor ◽  
Square Planar ◽  
Coordination Plane

The reaction of K2PtCl4 with CH3—CH=CH—CH2—OH yields the complex cis-[PtCl2((CH2=CH—CH(CH3))2O)]. The crystals are triclinic, space group [Formula: see text], a = 9.420(2) Å, b = 8.359(4) Å, c = 7.837(4) Å, α = 91.10(4)°, β = 62.13(4)°, γ = 80.80(5)°, and Z = 2. The structure, solved by standard methods, has been refined anisotropically by full matrix least-squares methods to a R factor of 0.052 by use of 2441 independent observed reflections. The complex is a monomer, where both double bonds of the diolefin ether are coordinated to the platinum atom as in Zeise's salt. The usual square planar coordination of platinum(II) is completed by two chlorine atoms. The (=CH2) groups of both double bonds are found on the same side of the coordination plane. Various possible conformations of the coordinated ligand in the complex are discussed.

Conformations of Bridged Diphenyls. VIII. Crystal Structure of 2-(2′,6′-Dinitrophenoxy)-t-butyIbenzene

1975 ◽  
Vol 53 (14) ◽  
pp. 2093-2101 ◽  
Author(s):  
Kapil Gurtu ◽  
W. David Chandler ◽  
Beverly E. Robertson
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Steric Effects ◽  
Monoclinic Space Group ◽  
X Ray Diffraction ◽  
X Ray ◽  
R Factor ◽  
Independent Molecules ◽  
Integrated Intensities

The crystal structure of 2-(2′,6′-dinitrophenoxy)-t-butylbenzene, C16HI5N2O5, has been determined by X-ray diffraction. The crystals are monoclinic, space group P21/c: a = 13.949(9), b = 9.652(6), c = 23.806(12) Å, β = 93.82(5), Z = 8. The integrated intensities of 6811 reflections were recorded with a four circle automated diffractometer at 20 °C; 3334 of these reflections were used in the refinement of the structure to a least-squares weighted residual of 0.057 and a traditional R factor of 0.057.The two crystallographically independent molecules both have the skew-t-butyl-distal conformation, suggesting that the steric effects of the two ortho-nitro groups play a greater role in determining the conformation than does conjugation with the bridging oxygen atom.

Crystal Structure of Synthetic Mg-Whitlockite, Ca18Mg2H2(PO4)14

1974 ◽  
Vol 52 (7) ◽  
pp. 1155-1164 ◽  
Author(s):  
Ramanathan Gopal ◽  
Crispin Calvo ◽  
Jun Ito ◽  
W. K. Sabine
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
Formula Unit ◽  
Full Matrix ◽  
Space Group ◽  
R Value ◽  
Unit Density ◽  
A Chain ◽  
Automatic Diffractometer

Crystals of synthetic Mg-whitlockite, Ca18Mg2H2(PO4)14, have been grown by hydrothermal techniques and their structure refined by full-matrix least-squares methods, using 1626 unique reflections measured with a Syntex [Formula: see text] automatic diffractometer, to a final R value of 0.046. The crystals have space group R3c with ZR = 1, a = 13.765(8) Å and α = 44.25(5)° with the equivalent hexagonal parameters a = 10.350(5), c = 37.085(12) Å and ZH = 3. The structure, although similar to that of βCa3(PO4)2, differs significantly. The structure contains interconnected infinite chains of polyhedra paralleling the hexagonal c axis with links in the chains consisting of three CaO8 polyhedra separated by two PO4 tetrahedra. Six of these chains surround a chain of MgO6 octahedra and PO4H groups which lie on the three-fold axes. These chains however contain only half the formula unit density of the calcium containing ones and a proton, presumably disordered, is attached to the oxygen atom on the triad axes.

Oxotetrafluoro-vanadate(V): Die Kristallstruktur von [enH2] [VOF4(H2O)]2.

1976 ◽  
Vol 31 (5) ◽  
pp. 541-543 ◽  
Author(s):  
Helmut Rieskamp ◽  
Rainer Mattes
Keyword(s):  
Crystal Structure ◽  
Hydrogen Bonds ◽  
Least Squares ◽  
Unit Cell ◽  
Monoclinic Space Group ◽  
Trans Position ◽  
Space Group ◽  
X Ray ◽  
In Trans ◽  
Oxygen Atoms

The crystal structure of [enH2][VOF4(H2O)]2 has been determined from X-ray diffractometer data. Crystals are monoclinic, space group C2/c with Z = 4 in a unit cell of dimensions a = 16.576(13), b = 7.781(4), c = 10.338(8) Å, β = 120.0(1)°.The structure was refined by least-squares methods to R 0.053 for 1436 reflections. The structure contains monomeric [VOF4(H2O)]⁻-ions with the oxygen atoms in trans position. The bond distances are 1.577 Å (terminal oxygen) and 2.333 Å (H2O molecule), resp. The V–F distances vary between 1.769(2) and 1.858(2) Å for fluorine atoms involved in strong hydrogen bonds.

[Na-15-Krone-5][MoF2Cl2(N3S2)]; Synthese und Kristallstruktur / [Na-15-Crown-5][MoF2Cl2(N3S2)]; Synthesis and Crystal Structure

1988 ◽  
Vol 43 (10) ◽  
pp. 1235-1239 ◽  
Author(s):  
Karin Völp ◽  
Gerhard Baum ◽  
Werner Massa ◽  
Kurt Dehnicke
Keyword(s):  
Crystal Structure ◽  
Ion Pairs ◽  
Sodium Atom ◽  
Acetonitrile Solution ◽  
Trans Position ◽  
Crystal Data ◽  
Synthesis And Crystal Structure ◽  
X Ray ◽  
In Trans ◽  
Ether Molecule

The cyclothiazeno complex [Na-15-crown-5][MoF2Cl2(N3S2)] has been prepared by the reaction of sodium fluoride with [MoCl3(N3S2)]2 in acetonitrile solution in the presence of [15-crown-5]. The compound was characterized by its IR spectrum as well as by an X-ray structure determination (3560 observed independent reflexions, R = 0.039). Crystal data: monoclinic, P21/n, Z = 4; a = 1044.8(2); b = 1513.7(2); c = 1363.8(3) pm; β = 104.33(2)°. The structure consists of ion pairs, in which the sodium atom is seven-coordinated by the oxygen atoms of the crown ether molecule and by the two fluorine ligands of the [MoF2Cl2(N3S2)]- unit. The molybdenum atom is a member of the planar MoN3S2 ring; the fluorine atoms are coordinated in trans position to the nitrogen atoms of the cyclothiazeno ring.

The crystal structure of [Pt(tetraethyldiethylenetriamine)I]I

1980 ◽  
Vol 58 (7) ◽  
pp. 664-668 ◽  
Author(s):  
Rosemary C. E. Durley ◽  
William L. Waltz ◽  
Beverly E. Robertson
Keyword(s):  
Crystal Structure ◽  
Least Squares ◽  
Structure Analysis ◽  
Three Dimensional ◽  
Crystal Structure Analysis ◽  
Unit Cell ◽  
Platinum Atom ◽  
Full Matrix ◽  
Square Planar ◽  
Dimensional Crystal

Crystals of [Pt(Et4dien)I]I, where Et4dien = (C2H5)2NC2H4NHC2H4N(C2H5)2, have been prepared. A three dimensional crystal structure analysis has been carried out in a monoclinic unit cell having a = 12.565(8), b = 7.576(6), c = 21.040(15) Å, β = 91.12(2)° and space group P21/c, Z = 4. Full-matrix least-squares using 1982 independent, observed reflections converged at R = 0.067. The platinum atom has square-planar co-ordination. The orientation of the four ethyl groups with respect to the plane of the ligand is similar to that observed in related molecules, in spite of a lack of similarity of the molecular packing. The iodide ion appears to be hydrogen bonded to the ligand.

Conformations of Bridged Diphenyls. X. Crystal Structure of 2-(4′-Carbomethoxy-2′-nitrophenylsulfinyl)-1,3,5-trimethylbenzene

1975 ◽  
Vol 53 (14) ◽  
pp. 2108-2114 ◽  
Author(s):  
Simon P. N. van der Heijden ◽  
W. David Chandler ◽  
Beverly E. Robertson
Keyword(s):  
Crystal Structure ◽  
Oxygen Atom ◽  
Least Squares ◽  
X Ray Diffraction ◽  
X Ray ◽  
R Factor ◽  
Oxygen Atoms

The crystal structure of 2′-(4′-carbomethoxy-2′-nitrophenylsulfinyl)-1,3,5-trimethylbenzene, C17H17NO5S, has been determined by X-ray diffraction. The crystals are triclinic, a = 9.848(11), b = 7.654(10), c = 12.513(15) Å, α = 107.33(8), β = 100.73(8), γ = 106.53(8)°, [Formula: see text] with Z = 2. The intensities of 3850 independent reflections were measured on a four circle diffractometer; 2985 reflections were used in the refinement to give a final least-squares residual of 0.053 and a traditional R factor of 0.052.Repulsion between the sulfoxide oxygen atom and the nitro oxygen atoms forces the molecule into the twist-nitro-proximal conformation as opposed to the nitro-distal conformation which has been observed for other bridged diphenyls in this series.

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